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WO2004087570A1 - Procede de production de nanotube en carbone - Google Patents

Procede de production de nanotube en carbone Download PDF

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Publication number
WO2004087570A1
WO2004087570A1 PCT/JP2003/004123 JP0304123W WO2004087570A1 WO 2004087570 A1 WO2004087570 A1 WO 2004087570A1 JP 0304123 W JP0304123 W JP 0304123W WO 2004087570 A1 WO2004087570 A1 WO 2004087570A1
Authority
WO
WIPO (PCT)
Prior art keywords
carbon
group
producing
compound
carbon nanotube
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2003/004123
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English (en)
Japanese (ja)
Inventor
Akio Kawabata
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujitsu Ltd
Original Assignee
Fujitsu Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fujitsu Ltd filed Critical Fujitsu Ltd
Priority to PCT/JP2003/004123 priority Critical patent/WO2004087570A1/fr
Priority to JP2004570174A priority patent/JP3973662B2/ja
Publication of WO2004087570A1 publication Critical patent/WO2004087570A1/fr
Priority to US11/155,494 priority patent/US7504570B2/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/152—Fullerenes
    • C01B32/156—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C01B32/162—Preparation characterised by catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/842—Manufacture, treatment, or detection of nanostructure for carbon nanotubes or fullerenes
    • Y10S977/843—Gas phase catalytic growth, i.e. chemical vapor deposition
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S977/00—Nanotechnology
    • Y10S977/84—Manufacture, treatment, or detection of nanostructure
    • Y10S977/842—Manufacture, treatment, or detection of nanostructure for carbon nanotubes or fullerenes
    • Y10S977/845—Purification or separation of fullerenes or nanotubes

Definitions

  • the present invention relates to a method for producing a carbon nanotube. More specifically, the present invention relates to a method for producing a carbon nanotube that can grow a carbon nanotube on a substrate by a CVD method without leaving carbon impurities.
  • an arc discharge method As a method for producing carbon nanotubes, an arc discharge method, a laser abrasion method, a thermal CVD method, a plasma CVD method, and the like are known.
  • the carbon nanotubes produced by the arc discharge and laser ablation methods consist of single-walled carbon nanotubes (SWNT: Single-Wall Nanotubes) with a single layer of graphene and multiple graphites.
  • SWNT Single-Wall Nanotubes
  • MWN T M a1 uti W all Nanotube.
  • MWNTs can be produced by the thermal CVD method and the plasma CVD method.
  • SWNT has a structure in which a single graphene sheet is assembled into a six-membered ring with strong bonds called sp 2 bonds between carbon atoms, and the tube end has a five-membered ring. Including several closed six-membered rings.
  • Japanese Patent Application Laid-Open Nos. H8-231210, JP-2000-1990, JP-T-2002-51518547, etc. disclose carbon nanotubes. Although purification methods are described, they are post-treatments after the production of carbon nanotubes and cannot be applied to carbon nanotubes produced directly on a substrate.
  • Japanese Patent Application Laid-Open No. 2000-86218 discloses that aromatic hydrocarbons such as benzene and toluene, or aliphatic hydrocarbons such as naphtha and light oil are used for the presence of a thermal decomposition accelerator such as sialic acid.
  • a thermal decomposition accelerator such as sialic acid.
  • Patent Document 1
  • Patent Document 2
  • Patent Document 4 Japanese Patent Laid-Open No. 2000-8662
  • An object of the present invention is to provide a method for producing carbon nanotubes, which can grow carbon nanotubes on a substrate by a CVD method without leaving carbon impurities.
  • the carbon nanotube production method of the present invention is a method for producing carbon nanotubes by growing carbon nanotubes on a substrate by a chemical vapor deposition (CVD) method using a reaction gas containing a compound of a carbon source.
  • CVD chemical vapor deposition
  • the compound of the carbon source is fullerene having the above functional group.
  • Preferred functional groups can have fullerene is a hydrogen atom, OH group, NO 2 group, NO 3 group, SO 3 group, S 0 4 groups, NH 2 groups, NH 3 group, NH 4 group, or a halogen atom is there.
  • the carbon source compound may be a hydrocarbon.
  • Hydrocarbons are> aliphatic hydrocarbons such as methane, acetylene, ethane, propane and butane, or cyclic hydrocarbons with aromatic rings (6-membered rings) such as benzene. Good.
  • Preferred functional group in which the carbon source compound can have hydrocarbons in an aliphatic hydrocarbon, NO 2 groups, N 0 3 group, SO 3 group, S 0 4 groups, NH 2 groups, NH 3 group, It is an NH 4 group or a halogen atom.
  • hydrocarbons in an aliphatic hydrocarbon NO 2 groups, N 0 3 group, SO 3 group, S 0 4 groups, NH 2 groups, NH 3 group, It is an NH 4 group or a halogen atom.
  • hydrogen atoms are also effective functional groups for removing carbon impurities.
  • FIGS 1A and 1B are diagrams showing the first half of the carbon nanotube manufacturing process according to the present invention described in Example 1.
  • FIGS. 2A and 2B are diagrams showing the latter half of the carbon nanotube production process according to the present invention described in Example 1.
  • the method for producing carbon nanotubes according to the present invention is a method for producing carbon nanotubes in which carbon nanotubes are grown on a substrate by a chemical vapor deposition (CVD) method using a reaction gas containing a compound of a carbon source. is there.
  • a feature of the present invention is to use a compound having a carbon skeleton and having a functional group effective for removing carbon impurities precipitated during carbon nanotube growth as a compound of a carbon source. .
  • Representative examples of the compound having a carbon skeleton in the present invention include fullerene of a carbon structure containing both a 5-membered ring carbon structure and a 6-membered ring carbon structure, or at least one carbon atom and hydrogen bonded thereto.
  • fullerene of a carbon structure containing both a 5-membered ring carbon structure and a 6-membered ring carbon structure, or at least one carbon atom and hydrogen bonded thereto.
  • carbon nanotubes can be grown according to the diameter and carbon arrangement of fullerene. It is also advantageous for the growth of carbon nanotubes to use cyclic hydrocarbons, especially benzene containing a ring structure similar to the six-membered ring constituting the carbon nanotube graph ensheet.
  • methane, acetylene, ethane, prono as usual. It is also possible to use lunar aliphatic compounds such as butane and butane as carbon sources. It is also possible to use a mixture of two or more carbon source compounds.
  • the carbon source compound used in the present invention needs to have at least one functional group effective for removing carbon impurities such as graphite-like substances and amorphous carbon that precipitate during the growth of carbon nanotubes.
  • fullerene carbon source compound consists essentially only carbon, is a functional group, a hydrogen atom, OH group, N0 2 groups, N0 3 group, SO 3 group, S 0 4 group, NH 2 group, NH Three groups, four NH groups, or halogen atoms can be used.
  • hydrocarbon containing hydrogen in addition to backbone carbon used as the carbon source compound functional groups, N0 2 groups, NO 3 group, S 0 3 group, SO 4 group, NH 2 group, NH 3 Group, NH 4 group, or halogen atom. If the hydrocarbon is a cyclic compound, hydrogen can also be considered a functional group.
  • Carbon impurities precipitated during carbon nanotube growth by the CVD method have higher reactivity than carbon nanotubes, and react with the functional groups contained in the carbon source compound under the growth conditions of carbon nanotubes to produce vapor. A high-pressure compound is generated, and this product is gasified to remove carbon impurities. As a result, carbon nanotubes can be grown by the CVD method while simultaneously removing carbon impurities.
  • Fullerenes with functional groups in other words, chemically modified fullerenes with functional groups, are readily available commercially.
  • Hydrocarbons with functional groups are also readily available commercially, or they can be synthesized.
  • a carbon compound having a functional group is used as a carbon source, but the growth mechanism of carbon nanotubes by the CVD method itself is the same as the growth mechanism when a normal carbon source without a functional group is used. It is considered to be basically the same as the mechanism. That is, by the action of the catalytic metal disposed on the substrate, the carbon supplied from the carbon source compound grows as a tube formed of a six-membered graphite sheet. At this time, carbon impurities such as amorphous carbon which tend to precipitate on the base material or the like are removed by being gasified by the action of the functional group as described above, and a clean carbon nanotube is obtained.
  • a more preferred carbon source compound in the present invention is fullerene.
  • Fullerenes come in a variety of diameters depending on the number of carbon atoms, such as 60, 84, 240, etc., that make up the fullerene molecule, and the diameter of the growing carbon nanotube is conveniently controlled according to the diameter be able to.
  • a fullerene having 60 carbon atoms has a diameter of about 0.7 nm, and using this as a nucleus, a carbon nanotube of this diameter can be grown.
  • fullerene is a carbon structure containing both a five-membered ring carbon structure and a six-membered ring carbon structure, and the five-membered ring structure has lower energy stability than the six-membered ring structure.
  • the five-membered carbon structure is broken, and a hemispherical nucleus is formed on the catalytic metal layer when all the bottoms of the fullerenes have become six-membered ring structures.
  • a carbon nanotube is formed based on such a nucleus, an armchair-type chirality nanotube is obtained. In this way, fullerenes By using this, it is easy to control the chirality of the growing carbon nanotube.
  • fullerene is a solid at room temperature and sublimates at high temperature to easily become a gas. Therefore, it is easier to handle than methane, acetylene, etc., which are gases at room temperature, and methanol, ethanol, etc. which are liquid at room temperature.
  • catalytic metal is used in the production of carbon nanotubes by the CVD method.
  • the catalyst metal transition metals such as Fe, Co, Ni, and Pd, or alloys of two or more thereof are used.
  • the catalytic metal can be disposed as a continuous layer on the growth substrate before the growth of the carbon nanotubes, or can be disposed as a number of fine particles.
  • the catalyst metal can be included in the molecule of the carbon source compound having a functional group. In this case, it is not always necessary to arrange the catalyst metal on the growth substrate.
  • a complex such as chlorocene modified with a functional group can be given. It is also possible to use a fullerene chemically modified with such a complex, or a fullerene chemically modified with each of a functional group and a catalytic metal.
  • the substrate on which the carbon nanotubes are grown according to the present invention may be a substrate of a semiconductor such as silicon-gallium arsenide (GaAs) or a substrate of an inorganic material such as quartz alumina.
  • a semiconductor such as silicon-gallium arsenide (GaAs)
  • GaAs silicon-gallium arsenide
  • quartz alumina an inorganic material
  • the CVD method used in the method for producing carbon nanotubes of the present invention may be a thermal CVD method or a plasma CVD method.
  • Example 1 As a carbon source compound having a functional group, C 60 fullerene (C 60 (OH) 12 ) chemically modified with an OH group is used. Sublimate C 60 (OH) 12 (or disperse in solvent and then boil to vaporize). As shown in Fig. 1A, thermal CVD with sublimated C60 (OH) 12 fullerene 10 placed on a silicon substrate 12 with a catalyst layer 14 formed on the surface by vapor-deposited Ni. Installed in a champ (not shown). By heating the inside of the champer to 600 ° C. at 1 kPa, C 60 (OH) 12 reacts with the Ni catalyst to produce nickel carbide. Subsequently, C 60 (OH) 12 is further supplied to grow carbon nanotubes 16 as shown in FIG.
  • C 60 (OH) 12 is further supplied to grow carbon nanotubes 16 as shown in FIG.
  • Carbon nanotubes are grown by thermal CVD using iron porphyrin containing Fe at the center of the porphyrin ring containing a benzene ring.
  • Iron porphyrin is introduced into a champer containing a silicon substrate (or a silicon substrate having a natural oxide film on the surface), and the inside of the chamber is heated to 500 ° at 1 kPa.
  • iron porphyrin is decomposed, and carbon nanotubes are grown on the substrate using Fe as a catalyst.
  • the carbon impurities precipitated at that time are removed by the action of hydrogen contained in the iron porphyrin, and a clean carbon nanotube can be obtained.
  • Carbon nanotubes are grown by thermal CVD using benzenesulfonic acid monohydrate C 6 H 5 SO 3 H ⁇ H 20 .
  • Benzenesulfonic acid monohydrate is introduced into a chamber containing a silicon substrate on which Ni is deposited (or a silicon substrate on which Ni is deposited on a natural oxide film on the surface).
  • benzenesulfonic acid monohydrate is decomposed, and carbon nanotubes are grown on the substrate using Ni as a catalyst.
  • the carbon impurities that are precipitated at that time are removed by SO 3 H of benzenesulfonic acid, and clean carbon nanotubes are obtained.
  • carbon nanotubes can be grown on a substrate by the CVD method without leaving carbon impurities. This can greatly promote the use of carbon nanotubes in semiconductor depises that are sensitive to the presence of impurities.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

La présente invention concerne un procédé de production d'un nanotube en carbone permettant de faire croître un nanotube de carbone sur un substrat par dépôt chimique en phase vapeur sans laisser d'impuretés de carbone. Avec ce procédé de production d'un nanotube de carbone on obtient la croissance du nanotube de carbone sur un substrat grâce à un procédé de dépôt chimique en phase vapeur (CVD) utilisant un gaz de réaction contenant un composé source de carbone. En l'occurrence, ce composé source de carbone présente un squelette de carbone pourvu d'un groupe fonctionnel réussissant à éliminer les impuretés de carbone pendant la croissance du nanotube de carbone.
PCT/JP2003/004123 2003-03-31 2003-03-31 Procede de production de nanotube en carbone Ceased WO2004087570A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
PCT/JP2003/004123 WO2004087570A1 (fr) 2003-03-31 2003-03-31 Procede de production de nanotube en carbone
JP2004570174A JP3973662B2 (ja) 2003-03-31 2003-03-31 カーボンナノチューブ製造方法
US11/155,494 US7504570B2 (en) 2003-03-31 2005-06-20 Method of manufacturing carbon nanotubes

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WO2007088829A1 (fr) * 2006-01-31 2007-08-09 Japan Science And Technology Agency Materiau portant un nanohorn de carbone et procede de synthese de nanotube de carbone
JP2009041140A (ja) * 2007-08-09 2009-02-26 National Institute Of Advanced Industrial & Technology 擬似円筒状単層中空炭素繊維
CN100482581C (zh) * 2005-06-17 2009-04-29 鸿富锦精密工业（深圳）有限公司 一种碳纳米管制造方法
US7781756B2 (en) * 2004-09-13 2010-08-24 Board Of Trustees Of The University Of Arkansas Nanotube-porphyrin molecular structure and applications of same
JP2012218949A (ja) * 2011-04-04 2012-11-12 Toyota Motor Corp カーボンナノチューブの製造方法
JP2018177562A (ja) * 2017-04-06 2018-11-15 アイシン精機株式会社 カーボンナノチューブ複合体の製造方法

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7781756B2 (en) * 2004-09-13 2010-08-24 Board Of Trustees Of The University Of Arkansas Nanotube-porphyrin molecular structure and applications of same
CN100482581C (zh) * 2005-06-17 2009-04-29 鸿富锦精密工业（深圳）有限公司 一种碳纳米管制造方法
WO2007088829A1 (fr) * 2006-01-31 2007-08-09 Japan Science And Technology Agency Materiau portant un nanohorn de carbone et procede de synthese de nanotube de carbone
JP5106123B2 (ja) * 2006-01-31 2012-12-26 独立行政法人科学技術振興機構 カーボンナノホーン担持体とカーボンナノチューブの合成方法
US8835006B2 (en) 2006-01-31 2014-09-16 Nec Corporation Carbon nanohorn carried material and process for producing carbon nanotube
JP2009041140A (ja) * 2007-08-09 2009-02-26 National Institute Of Advanced Industrial & Technology 擬似円筒状単層中空炭素繊維
JP2012218949A (ja) * 2011-04-04 2012-11-12 Toyota Motor Corp カーボンナノチューブの製造方法
JP2018177562A (ja) * 2017-04-06 2018-11-15 アイシン精機株式会社 カーボンナノチューブ複合体の製造方法
JP7024202B2 (ja) 2017-04-06 2022-02-24 株式会社アイシン カーボンナノチューブ複合体の製造方法

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US7504570B2 (en) 2009-03-17
JP3973662B2 (ja) 2007-09-12
US20070003471A1 (en) 2007-01-04
JPWO2004087570A1 (ja) 2006-06-29

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